Starch dispersion and a method of making it



Patented Feb. 10, 1948 2,435,961- STARCH DISPERSION stir) A; M'iirfibii "or" MAKING rr Allen F. Peters, Philadelphia; Pa;

N Drawing. Application desserts, ibis:

Serial No. 612;123

13 Claims. (cries-2n) The object of the-invention is to provide improvements in prepared starches of the type used both domestically and commercially for the 'sizing and stifiening of various fabrics, this application being a continuation-in-part of Serial No.- 469,135, filed December 15,- 1942*(abandoned).

Heretofore, with few if any'exceptions, laundry starch either in lump or powder form has always been cooked in water, and if necessary, thinned to the proper consistency, but inevitably a fresh batch has had to be made foreach requirement. This has been due principally to the fact that Ordinary cooked starch cannot-be kept for any length of time, asit tends to separate from the water inwhich it is initially dispersed, becomes rancid and molds easily from Organisms in the air, frequently changes in color to various shades of purple in bright sunlight, and so has not been considered as being adaptable to marketing in prepared condition.

Another and more specific object is to provide a starch product that can be kept for indefinite periods without deterioration or'other change in or from its original and essentially desirable characteristics, even when subjected to relatively high or low temperatures; and irrespective of whether it is stored in bulk, or preserved in bottles, cans or other containers as sci-called shelf goods. In fact, it has been subjected to temperatures" as high as the boiling point orwater (at sea level) and to temperatures" near the freezing point of water, without changing its usefulness to the slightestdegree, especially as regards such changes as usually result from either or both or these relatively extreme conditions;

A stillfurther object is to provide a thoroughly homogeneous starch product o'fthis character, which can be preparedarid marketed in a con sistency suitable for stiff laundry work, or which by varying the degree of dilution of thinning with water from and available source is'made instantly adaptable-for stiff laundrywork such as collars, cuffs, dress shirt bosoms and the like, s emi-stifi laundry work; such as negligee shirts, shirt waists and the like; also the-sizing of yarn, piece goods, manufactured clothing, upholsterifig and drapery materials and the like.- The only requirement for preventing the prepared starch from possible physical change; and anundes'irable degree of increased stifin'ess resulting-from evaporation, is that it shall be corked-or otherWi's ndainta-lned air-tight, as for instance after a portion has been used froma-giVencontainer.

And 22- Still:- fur-the! object is-to provide an" proved starch: product by means or a method;

which is'particularly characterized by the formal tion or a soa within the starch mass in Sitligl: e.; coincident with assembly or ihterniixing 0f the elements during processing, the combination thus effected producing a homogeneous dispersion of the starch and soap, so that no separation takes place when diluted for use parse; or coinbina tionwith the other ingredients:

Towards an understanding or the process by which theimproveu starch product oreclosed; the preparation of a orient-re unit will be HE- scribed iri' accordanee' withthe basic formulas stated below Beta pine oil I M cubic centimeters Solution sodium; silicate (cominercial1y available)= doe 5 to 15 Water to make 1 liter.

In preparing new product, approkimately 1191c gas of suitable cry eeinmerci i smug is first n'ii-ii'd thoroughly with about ea, or and water, and 'resuiniii mixture is their addedslowly to abo #650 cc; ofboiling water- (preferably contair ii a suitable soluble me: servatlve, such es sodium; benzoate; or chlorthymol', fornialdehyde, or benjzoici acidfor' prel-j veritioii' of mol s or rennentatidn),wm1e a small -'1'5 'cc.) is used to-riiise s e sani l l the t s m x The ridt's'taicn is mixed wen; em: while rice, potatoes, arrow root, sago, et cetera, canbe used with varying results, starch from corn is preferred, particularly on the basis of uniform-- ity, cheapness and availability.

This method produces the improved product 7 in its preferred form, as given in Formulas II and III. However, within the scope of the in- I vention is the preparation of a soap-and-starch product containing neither a preservative nor the beta pine oil, but maintaining the fundamental characteristic ,of having the starch remain in complete homogeneous suspension, as suggested by Formula I, and the soap formed in situ as the reaction product of stearic acid and triethanolamine. ,It ,might also be stated that in the manufacture of starch from its natural source, it is not necessary to thoroughly dry and sieve the starch for use in this preparation. It is necessary, however, to know by analysis the percentage of moisture content, so as to be able to calculate the amount of starch necessary or equal to the dry starch in the formula. The wet starch is mixed with cold water toform a uniform dispersion and the procedure from this point is the same as stated above.

A minimum temperature of 100 C. is preferable, as-stated; in order to produce the desired results in a minimum of time. The upper limit ofoptimum range is, therefore, given as approximately 105 C.- As long as the temperature or heating is not sufilciently high to cause charring, or produce a discoloration or other undesirable characteristics of the product, the heating being preferably by-means of live steam, as for instance a pressure cooker, hot water or steam-jacketed boiler.

After this step is completed, and while the starch is still hot, melted stearic acid 5 gm., is added and mixed thoroughly; To this mixture is added 6 cc. of triethanolamine dispersed in 30 cc. of hot water. Thorough mixing is essential at this point in order to insure complete and uniform dispersion of the triethanolamine-stearate soap as it isformed with the mixture, together with the excess triethanolamine. Other soaps may be formed within the liquid starch mass, in each case with preferably but not necessarily a slight excess of alkalinity in the product, depending upon the particular soap made. Such other soaps are represented by oleic acid and sodium hydroxide or mixed isopropanolamines, palmitic acid and potassium hydroxide or borax.

The product thus formed, preferably with the addition of the beta pine oil hereinafter referred to,' is satisfactory in every way commercially. However, a slightly improved product may be made by adding a salt such as sodium chloride, calcium chloride, magnesium chloride or magnesium sulphate, as for example a solution of 50 gm. of sodium chloride, either alone or with 5-10 gm. of alum, preferably ammonium alum, dissolved in 160 cc. of boiling water, while continuing tostir the mass. Thorough mixing is essential at this point, after which the product is either cooled by means of a water bath, or other suitable method, or allowed to cool to room temperature, preferably covered.

When the product, either with or without the inclusion of the salt and alum, has cooled to ap proximately 50 C., or to room temperature; a wetting agent such as glycerin, mineral oil, methyl salicylate, or preferably beta pine oil, 6 cc. to 10 cc. is added and thoroughly incorporated by mechanical stirring, which with water to form one liter completes the formula.

The purpose of the triethanolamine-stearate,

alum and sodium chloride is that they produce a gloss on the treated fabric when ironed, give to the fabric the property of being extraordinarily easy to iron, and also prevents the starch from -.-sticking to the flat iron or equivalent heated ele- "mentj'wherefore said compounds primarily represent any one or more of possibly a large group of substances suitable for the same purposes, such as sodium oleate, potassium alum and calcium chloride or potassium palmitate, iron alum and magnesium chloride. In addition, the triethanolamine-stearate, sodium chloride, and alum increase the property of being readily and easily dispersed uniformly in water.

A slight excessof triethanolamine over and above that needed to react with the stearic acid is used, this excess upon reacting with the alum forming a dispersible, possibly colloidal, com: pound. The last mentioned compound and methanolamine-stearate cooperate to maintain a uniform dispersion in the product which does not separate or show a separation of water, while aside from aiding in the ease with which the starch product can be mixed with water, also aids in forming a uniform dispersion of all of the ingredients in the product when mixed with water. This function of the soap is definitely increased to a maximum by forming it within the starch mass, as hereinbefore described, rather than attempting to form the soap externally and then mixing it with the starch solution or mass.

Triethanolamine soap, together with the excess of triethanolamine is of further importance due to the fact that it is also a wetting agent and increases the penetrating properties of the product along with the beta pine oil, which is also a. wetting, penetrating, preserving and aromatizing agent. The presence of a wetting agent increases the value of the product from the standpoint of thoroughly penetrating all fabrics, while increasing the ease with which a uniformly starched product or material is produced with a minimum of labor and time.

So far as the improved liquid sta'rch or starch paste is concerned, the formula is now completed and should be strained to remove any lumps or other particles that may be in the starch product, after which it maybe bottled or packaged without further treatment. It is to be understood that aromatizing agents such as methyl salicylate, oil of lavender, oil of peppermint, etc., may be added.

To any the basic formulas alone, or with either or both of the salt and alum added thereto, there may be further added a wax (1-3 gms.), such as paraffin, beeswax, spermaceti, or ozokerite. Again, to said basic formulas either alone or with any of the foregoing, and particularly those including the salt and/or the alum, there may be added zinc stearate. Additionally, the use of a small quantity of any of these starch products in the washing water serves as a cleansing agent, to augment the soap per se which is used only as a cleanser in that the starch mixture accelerates amen:

the separation-oithedirtfrom thesoiled fabrics.

If desire the product can be still further improvedjfroma commercial standpoint and accordingly rovide for its useas a single compound. instead of the two separate preparations comprising the usual freshly made liquid starch and bluing. For such acombination product, 0.5 gram to 5.0grams of a good gradeof bluing isvadded, either before or after the mass has cooled; to atmospheric temperature, the proportion. of bluing being dependent upon the quality and density of the same, as. said bluing. in noway affects the characteristics of the starchper se, as an independent article of commerce. and industry. Otherwise, the productis readyfor storage and use as many times as may be desired. ."In the matter of ingredients, proportio11S..temperatures, sequences; of formulations, and method, it is to be understood that these may be varied within such limits as are not precluded by definite specification herein to the contrary.

Among the distinct advantages noted as resulting from the use of the improved starch product, fabrics treated with it do not tend to Wrinkle as easily as similar materials treated with ordinary starch; in the event that water is splashed upon the iron fabric, there is a distinct tendency to shed such water instead of absorbing it, exactly as though the fabric had been definitely treated to make it Water-repellant; while in addition fabrics treated with the improved product are definitely less harsh, sharp and scratchy to the skin, than materials treated with ordinary starches. The fabrics, in short, have been pronounced as possessing a velvety or soft stiffness.

Having thus described my invention, what I claim and desire to protect by Letters Patent of the United States is:

1. The process of preparting a homogeneous, semi-liquid starch dispersion for use on textiles, which consists in mixing approximately 100 to 119.8 gm. dry starch with 150 cc. unheated water, adding the resulting mixture to approximately 650 gm. boiling water containing approximately gm. of a soluble preservative, continuing the resulting mixture at a temperature approximating the boiling point of water for approximately ten to fifteen minutes, adding approximately 5 gm. melted stearic acid, forming a soap in situ within the mixture by then adding approximately 6 cc. triethanolamine dissolved in hot water, permitting the mixture to cool, and finally adding approximately 10 cc. beta pine oil and sufiicient water to make one liter.

2. The process of preparing a homogeneous starch dispersion which consists in mixing approximately 100 to 119.3 gm. dry starch with 150 cc. unheated water, adding the resulting mixture to approximately 650 gm. boiling water containing approximately 5 gm. of a soluble preservative, continuing the resulting mixture at a temperature approximating the boiling point of Water for approximately ten to fifteen minutes, adding approximately 5 gm. melted stearic acid, forming a soap in situ within the mixture by then adding approximately 6 cc. triethanolamine dissolved in hot water, permitting the mixture to cool, and finally adding sufficient water to make one liter.

3. The process of preparing a homogeneous, semi-liquid starch dispersion for use on textiles, which consists in mixing dry starch with unheated water, adding the resulting mixture to boiling water containing a soluble preservative, continuing the resulting mixture at a temperature approximating the boiling point of water ifor approximateiy ten to fifteen minutes, adding meltedl'stearic acid, forming a. soap in situ within the mixture .by'then adding an excessv of triethanolamine dissolved in hot water, permitting the mixture to cool, and finally addingbeta pine. oil and suflicient water to make one liter.

4. The process of preparing a homogeneous starch dispersionwhich consists in mixing dry starch withunheated'water, adding the resulting mixture 'to boi l-in water containing a soluble preservative, continuing the resulting mixture at a temperature approximating the boiling point of water-ion approximately ten to fifteen minutes, adding melted stearic acid, forming a soap in situ within the mixture by then adding an excess of triethanolamine dissolved in hot water, permitting the mixture to. cool, and finally adding sufiicient water to make one liter.

5. A homogeneous prepared starch for use on textiles, comprising a semi-liquid dispersion of starch, sodium benzoate, the reaction product of stearic acid and an excess of triethanolamine formed in situ and zinc stearate.

6. A homogeneous prepared starch for use on textiles, comprising a semi-liquid dispersion of starch, approximately 2.5 gm. to 5 gm. sodium benzoate, the reaction product of 5 gm. stearic acid, and approximately 6 cc. to 10 cc. triethanolamine in combination, formed in situ 10 cc. beta pine oil, 5 to 15 cc. commercial solution sodium silicate, and water to make one liter.

7. The process of preparing a homogeneous starch dispersion, which consists in mixing dry starch with unheated water, heating to approximately the boiling point, adding melted stearic acid, forming soap in situ within the mixture by then adding triethanolamine dissolved in hot water, and then permitting the mixture to cool.

- 8. The process of preparing a homogeneous starch dispersion, which consists in mixing dry starch with unheated water, heating to approximately the boiling point, adding melted stearic acid, forming soap in situ within the mixture by then adding triethanolamine dissolved in hot water, adding an alkali forming metal chloride and alum, and then permitting the mixture to cool.

9. The process of preparing a homogeneous starch dispersion, which consists in mixing dry starch with unheated water, heating to approximately the boiling point, adding melted stearic acid, forming soap in situ within the mixture by then adding triethanolamine dissolved in hot water, adding an alkali forming metal chloride and then permitting the mixture to cool.

10. The process of preparing a homogeneous starch dispersion, which consists in mixing dry starch with unheated water, heating to approximately the boiling point, adding melted stearic.

acid, forming soap in situ within the mixture by then adding triethanolamine dissolved in hot water, adding alum, and then permitting the mixture to cool.

11. The process of preparing a homogeneous starch dispersion, which consists in mixing dry starch with unheated water, heating to approximately the boiling point, adding melted stearic acid, forming soap in situ within the mixture by then adding triethanolamine dissolved in hot water, adding a wax selected from the group consisting of parailin, beeswax, spermaceti and ozokerite, and then permitting the mixture to cool.

12. A homogeneous prepared starch for use on textiles, comprising a semi-liquid dispersion 01 7 starch, a presewative, the reaction product or .stearicacid and an excess of triethanolamine formed in situ, an alkali forming metal chloride I the group consisting of paraflin, beeswax, spermaceti and ozokerite.

ALLEN F. PETERS.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED-STATES PA'rENrs Number Name Date 158,104 Marney Dec. 22, 1814 1,183,829 Boyce May 16, 1916 2,228,784 Spilka Jan. 14, 1941 2,230,656 Scholler et a1. Feb. 4, 1941 2,250,115 Mayer et a1. July 22, 1941 2,280,699 Grant et al Apr. 21, 1942 2,321,244 Rawling June 8, 1943 2,350,653 Walsh June 6, 1944 FOREIGN PATENTS Number Country Date 431,275 Great Britain July 7, 1935 OTHER REFERENCES Industrial Solvent, Mellan-Reinbold Publishing 00., 1939, pp. 143, 144, 146 and 147. 

